反应详情

2-(2-Dimethylaminomethyl-5-furylmethylthio)ethylamine (4.00 g) and 2-nitroamino-5-[1-(2-dimethylaminoethyl)-2-oxopyridin-4-yl-methyl]pyrimidin-4-one (7.14 g) were refluxed in pyridine (50 ml) for 24 hours. The reaction mixture was evaporated under reduced pressure and the residue subjected to medium pressure column chromatography (Kieselgel 60 silica mesh - main column) using ethyl acetate:methanol (80:20→70:30) gradient elution. The fractions containing the desired title product were evaporated in vacuo and treated with maleic acid (1.79 g) in isopropanol. The solvent was evaporated under reduced pressure and the residue washed with acetone and cold isopropanol. On standing at 5° C. the residue crystallised from ethanol-methanol to yield 2-[2-(2-dimethylaminomethyl-5-furylmethylthio)ethylamino]-5-[1-(2-dimethylaminoethyl)-2-oxopyridin-4-ylmethyl]pyrimidin-4-one as a maleate salt (0.79 g), m.p. 123°-126° C.

1. customThe reaction mixture was evaporated under reduced pressure
2. washethyl acetate:methanol (80:20→70:30) gradient elution
3. additionThe fractions containing the desired title product
4. customwere evaporated in vacuo
5. additiontreated with maleic acid (1.79 g) in isopropanol
6. customThe solvent was evaporated under reduced pressure
7. washthe residue washed with acetone and cold isopropanol
8. customOn standing at 5° C.
9. customcrystallised from ethanol-methanol